CN108441666B - Ti2Preparation method of AlC particle reinforced copper-based composite material - Google Patents
Ti2Preparation method of AlC particle reinforced copper-based composite material Download PDFInfo
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- CN108441666B CN108441666B CN201810194151.3A CN201810194151A CN108441666B CN 108441666 B CN108441666 B CN 108441666B CN 201810194151 A CN201810194151 A CN 201810194151A CN 108441666 B CN108441666 B CN 108441666B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
- C22C1/1026—Alloys containing non-metals starting from a solution or a suspension of (a) compound(s) of at least one of the alloy constituents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C32/00—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
- C22C32/0047—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
- C22C32/0052—Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only carbides
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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Abstract
The invention discloses a Ti2AlC particle reinforced copper-based composite materialA preparation method of a material belongs to the field of composite material preparation, and comprises the specific steps of preparing Ti2AlC particle suspension; then carrying out surface treatment on the oxygen-free pure copper plate in the complete annealing state; then dispersing the Ti2Spraying AlC particle suspension on the surface of copper plate uniformly, superposing the two copper plates, fastening, rolling, cutting, repeating above steps for several times, and continuously adding Ti2AlC particles; and finally, continuously carrying out accumulative pack rolling on the plate for multiple passes. The preparation method of the invention can obviously improve the dispersibility of the reinforced particles in the matrix, obviously improve the hardness and strength of the composite material through the synergistic effect of particle reinforcement, fine grain reinforcement and work hardening, and simultaneously does not obviously reduce the conductivity of the composite material. The preparation method of the invention has the advantages of easy operation, simple process and low cost, and can be used for batch production.
Description
Technical Field
The invention belongs to the field of composite material preparation, and particularly relates to Ti2A preparation method of an AlC particle reinforced copper-based composite material.
Background
With the rapid development of industries such as machine manufacturing, electronic communication, rail transit, instrument and instrument, military industry and the like, people have higher and higher requirements on the strength, the electric conductivity, the heat conductivity, the fatigue and other properties of copper and copper alloy.
The strength and wear resistance of the matrix can be effectively enhanced by adding a reinforcing phase (ceramic particles, whiskers, fibers, carbon nanotubes, graphene and the like) into copper and copper alloys. Generally, as the content of the reinforcing phase increases, the mechanical properties of the copper-based composite material increase, but when the content of the reinforcing phase is higher, the electrical conductivity of the composite material is significantly reduced.
Therefore, the problem of how to greatly improve the strength and hardness while maintaining a higher conductivity level has been a central task in the research and development of copper-based composites. Ternary layered Ti2AlC ceramic particlesThe copper-based composite material not only has the properties of metal, but also has good heat-conducting property and electric conductivity, and also has the properties of ceramic, high melting point, high thermal stability and good oxidation resistance, thereby being an ideal reinforcing phase of a high-performance copper-based composite material.
The traditional powder metallurgy, casting, spray deposition and other processes can not effectively solve the problem of Ti2The problem of dispersion of AlC particles in a copper matrix material, which directly affects Ti2The reinforcing effect of the AlC particles further influences the electrical and mechanical properties of the composite material.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects in the prior art, the invention aims to provide Ti2The preparation method of the AlC particle reinforced copper-based composite material can not only obviously improve the dispersibility of the reinforced particles in a matrix, but also obviously improve the hardness and strength of the composite material and simultaneously not obviously reduce the conductivity of the composite material.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the following technical scheme:
ti2The preparation method of the AlC particle reinforced copper-based composite material comprises the following steps:
the method comprises the following steps: mixing Ti2Placing AlC particles into a mixed solution of alcohol and acetone, and preparing the Ti with good dispersion after high-speed dispersion2AlC particle suspension;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: dispersing Ti2Spraying AlC particle suspension on the surface of the treated pure copper plate uniformly, then laminating a layer of pure copper plate on the surface, fastening, rolling, cutting into halves, repeating the above processes, and continuously spraying Ti2AlC particles, sprayed Ti2The AlC volume fraction is 2-4% of that of the pure copper plate, and the plates are obtained by carrying out accumulated rolling for multiple passes;
step four: no more Ti is added2Continuing to perform different passes of accumulated rolling on the plate obtained in the third step to obtain Ti with uniform structure2The AlC particles reinforce the copper-based composite material.
Preferably, in the first step, the high-speed dispersion time is 30-60 min.
Preferably, in the first step, the volume ratio of the alcohol to the acetone is 1: 2.
preferably, in the step one, Ti is used2The particle size of the AlC particles is 100-200 nm.
Preferably, in the third step, the cumulative rolling pass is 2 to 4 times.
Preferably, in the third step, the reduction per pass in the cumulative rolling is about 55 to 65%.
Preferably, in the fourth step, the cumulative rolling pass is 4 to 6 times.
Preferably, in the fourth step, the reduction per pass in the cumulative rolling is about 50%.
Preferably, in the third step and the fourth step, the accumulated rolling process is not preheated and lubricated, and the rolling speed is 0.34 m/s.
Has the advantages that: compared with the prior art, the invention applies the accumulative pack rolling technology for preparing the ultrafine grained metal plate to prepare the particle reinforced copper-based composite material, can obviously improve the dispersibility of the reinforced particles in a matrix, obviously improves the hardness and strength of the composite material through the synergistic action of particle reinforcement, fine grain reinforcement and work hardening, and does not obviously reduce the conductivity of the composite material; by regulating and controlling Ti2The content of AlC particles, the rolling reduction and the rolling pass realize the controllable preparation of the microstructure and the performance of the material; the equipment required by the material preparation method is a conventional industrial rolling mill, the preparation method is easy to operate, the process is simple, the cost is low, and batch production can be carried out.
Detailed Description
The technical solution of the present invention is further described below with reference to examples.
Ti2The preparation method of the AlC particle reinforced copper-based composite material comprises the following steps:
the method comprises the following steps: mixing Ti2AlCThe particles are put into a mixed solution of alcohol and acetone, and dispersed at high speed to prepare well dispersed Ti2AlC particle suspension;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: dispersing Ti2Spraying AlC particle suspension on the surface of the treated pure copper plate uniformly, then laminating a layer of pure copper plate on the surface, fastening, rolling, cutting into halves, repeating the above processes, and continuously spraying Ti2AlC particles, sprayed Ti2The AlC volume fraction is 2-4% of that of the pure copper plate, and the plates are obtained by carrying out accumulated rolling for multiple passes;
step four: no more Ti is added2Continuing to perform different passes of accumulated rolling on the plate obtained in the third step to obtain Ti with uniform structure2The AlC particles reinforce the copper-based composite material.
In the first step, the high-speed dispersion time is 30-60 min.
In the first step, the volume ratio of the alcohol to the acetone is 1: 2.
in the step one, the Ti2The particle size of the AlC particles is 100-200 nm.
In the third step, the accumulated rolling pass is 2-4 times.
In the third step, the reduction of each pass is about 55-65% during the accumulative pack rolling.
In the fourth step, the accumulated rolling pass is 4-6 times.
In the fourth step, the reduction per pass in the cumulative pack rolling is about 50%.
In the third step and the fourth step, the accumulated rolling process is not preheated and lubricated, and the rolling speed is 0.34 m/s.
Example 1
This example was conducted to add 2 vol% Ti2Preparation of Ti by AlC particle accumulation and pack rolling2For AlC particle reinforced copper-based composite material, the size of the oxygen-free pure copper plate is 200mm × 25mm × 1mm, and the Ti is2The size of the AlC particles is 100-200 nm. The Ti2AlCThe preparation method of the particle reinforced copper-based composite material comprises the following steps:
the method comprises the following steps: 0.45g of Ti2Dispersing AlC particles in 200ml mixed solution of alcohol and acetone at high speed for 30min to obtain Ti2AlC particle suspension;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: half of the well dispersed Ti2Spraying AlC particle suspension liquid on the surface of the copper plate uniformly, overlapping, fastening, rolling and shearing the two copper plates, repeating the above processes, and adding Ti2Carrying out 2 passes of accumulated rolling on the AlC particles, wherein the reduction of each pass is about 60%;
step four: no more Ti is added2And C, carrying out accumulative pack rolling on the plate obtained in the step three to 6 times, wherein the reduction of each time is about 50%.
Example Ti2The properties of the AlC particle reinforced copper-based composite material are shown in table 1: the conductivity at room temperature was 93.5%; microhardness of 135.33Hv0.05Pure copper in the as-annealed state (50.88 Hv)0.05) 2.69 times of; the tensile strength is 489.56MPa, which is 2.22 times of the original annealed pure copper (220.67 MPa).
Example 2
This example was conducted to add 2 vol% Ti2Preparation of Ti by AlC particle accumulation and pack rolling2For AlC particle reinforced copper-based composite material, the size of the oxygen-free pure copper plate is 200mm × 25mm × 1mm, and the Ti is2The size of the AlC particles is 100-200 nm. The Ti2The preparation method of the AlC particle reinforced copper-based composite material comprises the following steps:
the method comprises the following steps: 0.45g of Ti2Dispersing AlC particles in 200ml mixed solution of alcohol and acetone at high speed for 30min to obtain Ti2AlC particle suspension;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: half of the well dispersed Ti2The AlC particle suspension is uniformly sprayed on the surface of the copper plate and thenSuperposing, fastening, rolling and cutting two copper plates, repeating the above processes, and adding Ti2Carrying out 2 passes of accumulated rolling on the AlC particles, wherein the reduction of each pass is about 60%;
step four: no more Ti is added2And C, carrying out accumulative pack rolling on the plate obtained in the step three to 8 times, wherein the reduction of each time is about 50%.
Example Ti2The properties of the AlC particle reinforced copper-based composite material are shown in table 1: the conductivity at room temperature was 93.2%; microhardness of 138.13Hv0.05(ii) a The tensile strength was 495.81MPa, which was 275.14MPa and 29.88MPa higher than that of the original annealed pure copper and the pure copper of the same pass (comparative example), and in addition, the strength was found to be saturated after 6 passes of the cumulative pass of the rolling in comparison with example 1.
Example 3
This example was conducted to add 4 vol% Ti2Preparation of Ti by AlC particle accumulation and pack rolling2For AlC particle reinforced copper-based composite material, the size of the oxygen-free pure copper plate is 200mm × 25mm × 1mm, and the Ti is2The size of the AlC particles is 100-200 nm. The Ti2The preparation method of the AlC particle reinforced copper-based composite material comprises the following steps:
the method comprises the following steps: 0.9g of Ti2Dispersing AlC particles in 400ml mixed solution of alcohol and acetone at high speed for 30min to obtain Ti2AlC particle suspension;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: dispersing Ti2Spraying AlC particle suspension liquid on the surface of the copper plate uniformly, overlapping, fastening, rolling and shearing the two copper plates, repeating the above processes, and adding Ti2Carrying out 4 passes of accumulated rolling on the AlC particles, wherein the reduction of each pass is about 60%;
step four: no more Ti is added2And C, carrying out accumulative pack rolling on the plate obtained in the step three to 8 times, wherein the reduction of each time is about 50%.
Example Ti2AlC particle reinforced copper-based composite materialThe properties of (A) are shown in Table 1: the conductivity at room temperature was 92.5%; microhardness of 147.24Hv0.05(ii) a The tensile strength was 483.45MPa, 17.52MPa higher than that of pure copper (comparative) in the same pass, comparable to that of example 1, indicating that as the reinforcing phase content increases, an increase in the pass is required to obtain a higher strength.
Example 4
This example was conducted to add 4 vol% Ti2Preparation of Ti by AlC particle accumulation and pack rolling2For AlC particle reinforced copper-based composite material, the size of the oxygen-free pure copper plate is 200mm × 25mm × 1mm, and the Ti is2The size of the AlC particles is 100-200 nm. The Ti2The preparation method of the AlC particle reinforced copper-based composite material comprises the following steps:
the method comprises the following steps: 0.9g of Ti2Dispersing AlC particles in 400ml mixed solution of alcohol and acetone at high speed for 30min to obtain Ti2AlC particle suspension;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: dispersing Ti2Spraying AlC particle suspension liquid on the surface of the copper plate uniformly, overlapping, fastening, rolling and shearing the two copper plates, repeating the above processes, and adding Ti2Carrying out 4 passes of accumulated rolling on the AlC particles, wherein the reduction of each pass is about 60%;
step four: no more Ti is added2And C, carrying out accumulative pack rolling on the plate obtained in the step three to 10 times, wherein the reduction of each time is about 50%.
Example Ti2The properties of the AlC particle reinforced copper-based composite material are shown in table 1: the conductivity at room temperature was 91.4%; microhardness of 149.57Hv0.05Pure copper in the as-annealed state (50.88 Hv)0.05) 2.94 times of; the tensile strength is 501.95MPa, which is 2.27 times of the original annealed pure copper (220.67 MPa).
Comparative example
Without addition of Ti2The AlC particles are produced by using annealed oxygen-free pure copper plates with the same size as a raw material and performing cumulative overlapping rolling on the raw material, wherein the preparation method comprises the following steps:
the method comprises the following steps: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step two: and (3) overlapping, fastening, rolling and half shearing the two copper plates, repeating the processes, and performing cumulative overlapping rolling for 8 passes, wherein the reduction of each pass is about 50 percent, and the rolling speed is 0.34 m/s.
The properties of the comparative pure copper plate were as follows: the conductivity at room temperature was 94.3%; microhardness of 125.67Hv0.05(ii) a The tensile strength was 465.93 MPa.
TABLE 1 results of comparison of comparative examples with examples 1 to 4
As can be seen from Table 1, Ti produced by accumulative pack rolling2The AlC particle reinforced copper-based composite material has high hardness and tensile strength, and 2 vol% of Ti in example 22The microhardness of the AlC particle reinforced copper-based composite material after 8 accumulated pack rolling passes is 138.13Hv0.05(ii) a The tensile strength was 495.81MPa, 275.14MPa and 29.88MPa higher than the original annealed pure copper and the pure copper of the same pass (comparative example), respectively, which is a synergistic result of grain strengthening, fine grain strengthening and work hardening. Albeit with Ti2The conductivity of the composite decreased with increasing AlC particle content, but 4 vol% Ti was present in example 42The conductivity of the AlC particle reinforced copper-based composite material after 10 accumulated pack rolling passes is still as high as 91.4%. Therefore, the accumulative pack rolling is a Ti for obtaining high strength and high conductivity2An ideal preparation method of the AlC particle reinforced copper-based composite material.
Claims (4)
1. Ti2The preparation method of the AlC particle reinforced copper-based composite material is characterized by comprising the following steps of: the method comprises the following steps:
the method comprises the following steps: mixing Ti2Placing AlC particles into a mixed solution of alcohol and acetone, and preparing the Ti with good dispersion after high-speed dispersion2Suspension of AlC particles, said Ti2The grain size of the AlC particles is 100-200 nm;
step two: carrying out surface treatment on the oxygen-free pure copper plate in a complete annealing state to remove surface oil stains and an oxidation film;
step three: dispersing Ti2Spraying AlC particle suspension on the surface of the treated pure copper plate uniformly, then laminating a layer of pure copper plate on the surface, fastening, rolling, cutting into halves, repeating the above processes, and continuously spraying Ti2AlC particle suspension, sprayed Ti2Ti in AlC particle suspensions2The AlC particles account for 2-4% of the volume fraction of the pure copper plate, and the plate is obtained by carrying out multiple passes of accumulative rolling, wherein the accumulative rolling passes are 2-4, and the reduction of each pass is 55-65%;
step four: no more Ti is added2Continuing the accumulated rolling of different passes on the plate obtained in the step three by using AlC particle suspension to obtain Ti with uniform tissue2The accumulated rolling passes of the AlC particle reinforced copper-based composite material are 4-6 times, and the reduction of each pass is 50%.
2. A Ti according to claim 12The preparation method of the AlC particle reinforced copper-based composite material is characterized by comprising the following steps of: in the first step, the high-speed dispersion time is 30-60 min.
3. A Ti according to claim 12The preparation method of the AlC particle reinforced copper-based composite material is characterized by comprising the following steps of: in the first step, the volume ratio of the alcohol to the acetone is 1: 2.
4. a Ti according to claim 12The preparation method of the AlC particle reinforced copper-based composite material is characterized by comprising the following steps of: in the third step and the fourth step, the accumulated rolling process is not preheated and lubricated, and the rolling speed is 0.34 m/s.
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Application publication date: 20180824 Assignee: Jiangsu Shenggong Construction Group Co.,Ltd. Assignor: YANCHENG INSTITUTE OF TECHNOLOGY Contract record no.: X2022980029965 Denomination of invention: A preparation method of Ti2AlC particle reinforced copper matrix composites Granted publication date: 20200731 License type: Common License Record date: 20230105 Application publication date: 20180824 Assignee: Jiangsu Jiujian Construction Engineering Co.,Ltd. Assignor: YANCHENG INSTITUTE OF TECHNOLOGY Contract record no.: X2022980028532 Denomination of invention: A preparation method of Ti2AlC particle reinforced copper matrix composites Granted publication date: 20200731 License type: Common License Record date: 20221230 Application publication date: 20180824 Assignee: SUNWAVE COMMUNICATIONS Co.,Ltd. Assignor: YANCHENG INSTITUTE OF TECHNOLOGY Contract record no.: X2022980028529 Denomination of invention: A preparation method of Ti2AlC particle reinforced copper matrix composites Granted publication date: 20200731 License type: Common License Record date: 20221230 |